CATIALO4 SPINAL CERAMIC NANO OVALS: SYNTHESIS, PHYSICOCHEMICAL CHARACTERIZATION AND ANTIMICROBIAL ACTIVITY WITH WATER REMEDIATION APPLICATION
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Research Journal of Chemistry and Environment_______________________________________Vol. 25 (6) June (2021)
Res. J. Chem. Environ.
CaTiAlO4 Spinal Ceramic Nano Ovals: Synthesis, Physicochemical
Characterization and Antimicrobial Activity with Water
Remediation Application
Patil M.V.1*, Bamane S.R.2 and Khetre S.M.3
1. Department of Chemistry, Miraj Mahavidyalaya, Miraj-416410, INDIA
2. Sushila Shankarrao Gadave Mahavidyalaya, Khandala, Satara-416416, INDIA
3. Department of Chemistry, Dahiwadi College, Dahiwadi, Satara-416416, INDIA
*
pramanikpatil@rediffmail.com
Abstract suitable nanocomposite mix metal oxide ceramic material to
Oval shaped CaTiAlO4 nanoparticles were synthesized by kill microbial contents of water resources to generate good
wet chemical co precipitation and muffle ignition method. quality of potable water6,11,15,30.
The oval shapes of nanomaterial were confirmed using SEM
imaging and spinal packing in crystals were determined on Hydrogen peroxide is the major theme for this application of
the basis of XRD spectrum. The surface functionalities over ceramic nanocomposites as these materials generate
nanomaterial was confirmed using FTIR spectrum peroxide entities with porous surface in water14. Oval
elucidating hydroxyl and oxide groups over surface for ceramic material can be used not only for antimicrobial
future water wetability. application but also for water remediation.
Furthermore the porous nature and electronic states in Material and Methods
nanomaterial were elaborated on the basis of UV-Vis. And All the chemicals used for synthesis for nanocomposites and
PL spectral transitions along with matching SEM and XRD their in vitro biological screening such as aluminium nitrate,
data. The very high porosity of this ceramic nanomaterial titanium chloride, calcium nitrate, conc. HCl and ethanol
was confirmed by BET measurements and future water were of A. R. grade. These chemicals were purchased from
remediation applications were demonstrated using S. D. Fine Chem. Ltd. and Merck and were used without
antimicrobial testing on Staphylococcus Aureus and further purification. The cell culture medium such as agar
membrane water purification activity. Overall this novel growth broth and bacterial culture, fetal bovine serum,
ceramic porous nano material has proved useful application trypsin buffer were obtained from Hi Media Ltd. The double
in water purification membranes. distilled water was obtained from Millipore system and used
throughout the synthesis and in vitro biological screening
Keywords: Oval ceramic, Nano material, Highly Porous, tests.
Water remediation, Absorbance.
General procedure
Introduction Synthesis of oval ceramic nanoparticles: All the metal
With the idea in the field of ceramic water nanotechnology, salts are mixed in 0.01M proportion in 25 ml. double
here in this research work we had developed a new class of distilled water and traces of HCL are added to the flask. The
trio oval metal oxide ceramic nanocomposite material for flask contents are vortexed on magnetic stirrer at 600 rpm.
microbial remediation of surface water resources. Calcium for 6 hours. Visible color change was observed after
and titanium based materials are used nowadays for formation of precipitate. The precipitate was washed with
antimicrobial applications in various fields.19,20,26,33 Along double distilled water and dried in oven at 92OC. The dried
with sodium it can form stable mix metal oxide to result in trio metal oxide nano composite ceramic powder was then
trio metal ceramic type material with good expected crushed and bonded with gluteraldehyde binder to form
porosity. Porosity is mainly important for water remediation pallet. This powder and pallet were characterized and used
and antimicrobial effects of bacterial cell adhesion. So here for antimicrobial studies in water remediation.
in this research work we had synthesized this mixed metal
oxide ceramic nanocomposite for such porosity required for Co-precipitation method: For this experimental detection,
antimicrobial effects and future water remediation co-precipitation method is used. The advantage of the co
applications.1,3,6 precipitation method involve simplicity and rapid
preparation, composition and particle size control, energy
Nano technology has emergent research fields which are efficiency, low temperature and homogeneity of particles.
growing towards development of new class of ceramic metal There are three main mechanism of co-precipitation:
oxide materials used for water remediation. Ceramic metal inclusion, occlusion and adsorption.
oxide nanoparticles and nano composites are having suitable
applications for antimicrobial and cleansing of water Structural and morphological characterization of oval
pollutants and agents. Limited number of reports have been nanomaterial: As mentioned in table 1, the structure,
attempted and published by researchers in this field.17,19,20 So morphology, particle diameter range and types of bonding of
there is need of development of new class of cheaper and functionalities in the ceramic nanocomposite was
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Res. J. Chem. Environ.
determined based on physicochemical characterization using the wells bored on plates. The gram positive Staphylococcus
UV-Vis., PL, FTIR, XRD spectrometry techniques and SEM Aureus bacteria was grown on culture plates and inhibited
microscopic analysis.2,8-10,36 The Spectronics double beam by dosing of material solutions in buffer dispersions with
UV-Vis. spectrometer with water as blank was used to physiological pH = 7.4 by use of phosphate buffer 26. The
determine absorption spectrum of material. culture plates were incubated and zones of inhibition were
measured and biocompatibility/ antimicrobial property of
To confirm functionalities present in material and comparing nanocomposite was elaborated.
with pallet form, Perkin Elmer series FTIR spectrometer was
used with KBr pellet technique. The PL emission spectrum Results and Discussion
of nanocomposite was determined using Jusco type spectra Morphological and structural characterization of
fluorometer with excitation identity of material with same 25 ceramic nanomaterial
ppm concentrations. The X-ray diffraction pattern of UV-vis Absorption and pl emission spectrum: The UV-
material was determined using X-ray spectrometer by vis region of energy for electromagnetic spectrum at
powder diffraction technique to elaborate the packing f ions, wavelength range from 200nm to 400nm. Absorbance or
hybridization and crystal system of nanocomposite entities. emission peak shown in fig. 1 of UV-Vis spectrum is due to
The composition of material, formation and phase of Schiff base transition21,24,25 results in metal CORM complex
ceramic nanocomposite is proved here by this spectrometric charge transfer transition. The UV-Vis absorption at 209.5
analysis. nm is due to n to pi absorption maxima in which charge
transfer takes place A1g to T1g and A2g to T2g from d5 state
Antimicrobial screening on gram positive bacteria by of Ti and Al for splitting from bonding of carbimide and CO
agar well disc diffusion method: The cell-particle species. PL g at 222 nm is due to n to Pi relaxation in which
interactions of materials demonstrating their reactivity and charge transfer takes place Pi to Pi relaxation- no quenching
biocompatibility can be elaborated using simple in vitro due to Ti, Al oxide.
antibacterial screening in buffer solutions to maintain
physiological mimicking pH at material cell interactions. As The composition of material, formation and phase of
cell pH affect on the biocompatibility of molecules. Here in ceramic nanocomposite was proved here by spectrometric
this work 20 ppm. concentrations of material were dosed on analysis.
bacterial cell cultures grown in agar broth on discs, inside
Figure 1: UV-Visible absorption spectrum of CaTiAlO4 ceramic nanomaterial
Table 1
MLCT transitions of non bonded/ Pi electrons of ligands and d electrons of metals
Absorption or emission peak Schiff base transition Metal CORM complex charge transfer
shown in UV-Vis. Or PL spectrum transition
UV-Vis. Absorption at 209.5nm. n to Pi absorption maxima A1g to T2g and A1g to A2g from d5 state of Ti ans Al
for splitting from bonding of carbimide and CO
species
PL g at 222 nm. n to Pi relaxation- Pi to Pi relaxation – no quenching due to Ti, Al
no quenching oxide
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Research Journal of Chemistry and Environment_______________________________________Vol. 25 (6) June (2021)
Res. J. Chem. Environ.
Figure 2: PL emmission spectrum of CaTiAlO4 disc Nanomaterial
Table 2
Matching of FTIR signals elaborating the functionalities of Schiff base and CORM complex
Signal in FTIR Functionality Ceramic group functionality
spectrum
483 cm-1 Ca-Al linkage Metal-oxide bonds
828 cm-1 Al-O linkage Presence of linked oxide metal species
1050 cm-1 Ti-Al group Metal (I) and Metal (III) interaction
1385 and 1663 cm-1 Presence of hydroxide Surface groups of oxide nanomaterial
1764 and 3222 cm-1 Presence of –OH and Oxides Presence of surface moisture for porosity
Figure 3: FTIR spectrum of CaTiAlO4 ceramic nanomaterial for surface functionalities
FTIR spectrum of ceramic nanomaterial for surface correspond to peak of (101), (221), (242), (211), (412). As
functionalities: FTIR spectrum of ceramic nanomaterial per XRD data in fig. 4, it has been proved that the ceramic
CaTiAlO4 is shown in fig. 3 and table 2. With the help of it nano composite material has octahedral packing of ions and
we can find surface groups.12,24,32 cubic phase purity elaborated 65nm size from main peak by
using Schere’s equation:
XRD (X- RAY diffraction) pattern of trio metal
nanomaterial: X-ray diffraction study of CaTiAlO4 ceramic d= a/√ h2+k2+12 (1)
nano material sample was examined by XRD analysis
10,13,35.Fig. 4 shows x-ray diffraction pattern of CaTiAlO As per XRD data in figure 3 and table 3, it had been proved
4
ceramic nano material sample analyzed at different that the ceramic nanocomposite has octahedral packing of
temperatures 0C. The XRD analysis of this sample contain ions and cubic phase purity elaborating the 65 nm sizes from
similar pattern with each other except change in peak height main peak using Scherer’s equation.
and peak with increase in temperatures. This pattern
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Research Journal of Chemistry and Environment_______________________________________Vol. 25 (6) June (2021)
Res. J. Chem. Environ.
SEM image for disc morphology: The SEM image of BET isotherm elaborating porosity of disc nanomaterial:
nanocomposite ceramic was shown in figure 5. It throws As per fig. 6, it is oberved that the ceramic nanocomposite
light on Oval shapes of material with some aggregation of show multi layer BET isotherm for nitrogen adsorpion hence
particles. This trio metal oxide ceramic composite possess it has good surface posrosity. The BET plot hence proved
not only porosity but also exhibits Oval shapes for better presence of porosity on surface of this nanocomposite
water loving nature and cell particle interactions. ceramic material.9
Table 3
Crystal parameters of Ceramic nanocomposite with octahedral packing matched with known ceramic JCPDS card.
0 0
Crystallite planes Lattice Constant
d Calculated A d Standard A 0
(Miller Indices) 2 2 2
JCPDS card no.- 86- a and b A from main XRD peaks
(h,k,l) d = a/√(h +k +l )
6788 for CaTiAlO4 [242] at theta = 37.5 of disc
Main peaks of ceramic or
matched ceramic nanomaterial
nano trio metal oxide 2dSinθ= nλ
101 4.324 4.345 a standard = 5.249
221 5.453 5.456 b standard = 7.266
242 7.234 7.230
211 4.986 4.988 a calculated = 5.251 and
412 6.789 6.785 b calculated = 7.272
Figure 4: XRD pattern of the disc CaTiAlO4 ceramic nanomaterial
Figure 5: SEM image of CaTiAlO4 nanomaterial with oval morphology
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Research Journal of Chemistry and Environment_______________________________________Vol. 25 (6) June (2021)
Res. J. Chem. Environ.
Antimicrobial properties for water remediation from nanocomposite exhibit antimicrobial and water remediation
nanomaterial: As per figure 7 and table 4, for antimicrobial potential at surface by material cell interactions. Here as
activity of 20 ppm material on Staphylococcus aureus, it had material had surface porosity after reaction with cell
been demonstrated that good zone of inhibition was having membrane material and water, the surface of material shows
better antimicrobial activity.26,36 adhesion to liquid and biomaterials which result in
dissociation of nanocomposite to oxides on surface,
Mechanism for antimicrobial activity and water resulting in production of peroxide on surface. This peroxide
remediation activity: As per physicochemical and produced at surface of nanomaterial further can produce
antimicrobial screening of material and elaboration in oxide and super oxide radicals to give antimicrobial effects
scheme 1, the disc nanomaterial trio metal oxide ceramic for water remediation activity.26,36
Figure 6: BET adsorption isotherm of CaTiAlO4 nanomaterial elaborating surface porosity
Figure 7: Anti microbial effects of ceramic nanomaterial on Staphylococcus Aureus for zone of inhibition at 20 ppm.
Table 4
Anti microbial activities of Schiff base and complex compared for gram positive and gram negative bacteria.
Type/ name of bacterial culture in Zones of inhibition for gram positive bacteria as zone diameter in
Agar broth mm. for Concentrations of drug/ dose of ceramic nanomaterial
[as per figures] At 10 ppm. At 25 ppm Fig. 7
Staphylococcus Aureus (gram +ve) 15 mm. 27 mm.
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Research Journal of Chemistry and Environment_______________________________________Vol. 25 (6) June (2021)
Res. J. Chem. Environ.
Water remediation activity of CaTiAlO4 characteristics wavelength. The percentage degradation of
Explanation: The photo catalytic degradation of methylene methylene blue dye at irradiated time interval was calculated
blue dye in CaTiAlO4 mixed oxide ceramic suspension by using following equation:
under UV light elimination was investigated in order to
evaluate its photo catalytic activity18,32. A reaction system At
Degradation Percentage = (1 − ) x 100
was setup at 20ppm concentration and 150 mg/100ml photo Ao
catalysts amount. Sample is observed in total 180 min in
photo catalytic multi lamp reactor with UV light (365 nm Hg where A is absorbance after time‘t’ and Ao is absorbance of
Vapor lamp) with maximum emission at about 660 nm at dye solution before degradation.
room temperature at constant starring to maintain
It has been observed that at 180 min. Methylene blue dye
homogeneous suspension. The suspension was irradiated for
30 min to 3 hrs. period. The suspension was withdrawn and shows 68% degradation rate. The absorption band gap of
centrifuge at each time of interval to remove CaTiAlO4 CaTiAlO4 is 3.63 eV indicating that ceramic nano catalyst
particles. CaTiAlO4 is suitable and best catalyst for degradation of
methylene blue dye result in removal of polluted elements
from water resources.
The absorption of methylene blue dye solution was
measured using UV-visible Spectrophotometer at its
Table 5
Degradation Parameters
1. Dye Methylene Blue
2. Concentration 20 ppm
3. Photo catalyst’s amount 150mg/100mL
4. Degradation Time 180 min
5. Degradation Efficiency 68%
6. pH 7
6. Source of light 365 nm Hg Vapor lamp
Fig. 8: % Degradation of Methylene Blue Dye with catalyst CaTiAlO4
Table 6
% degradation during course of time
Time % Degradation of MB
Blank 00
Adsorption 5
30 min 19
60 min 33
90 min 42
120 min 66
150 min 67
180 min 68
168Research Journal of Chemistry and Environment_______________________________________Vol. 25 (6) June (2021)
Res. J. Chem. Environ.
Fig. 9: Absorbance Band gap of CaTiAlO4
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